Nanostructured powders and related nanotechnology

• US 7,081,267 B2
• Filed: 07/08/2003
• Issued: 07/25/2006
• Est. Priority Date: 09/03/1996
• Status: Expired due to Term

• Current Assignee: PPG Industries Ohio Incorporated (Nouryon BV)
• Original Assignee: NanoProducts Corporation (Nouryon BV)
• Inventors: Yadav, Tapesh
• Primary Examiner(s): Kalafut, Stephen J.
• Application Number:
  US10/614,845
• Publication Number:
  US 20040005485A1
• Time in Patent Office: 1,113 Days
• Field of Search: 427/115, 427/124, 427/126.1, 427/248.1, 427/250, 427/2, 429/30, 429/40, 264/12
• US Class Current: 427/115
• CPC Class Codes: B01J 12/005 carried out at high temperatures, e.g. by pyrolysis
• CPC Class Codes: B01J 12/02 for obtaining at least one reaction product which, at normal temperature, is in the solid state
• CPC Class Codes: B01J 19/24 Stationary reactors without moving elements inside B01J19/08, B01J19/26 take precedence; with stationary particles B01J8/02
• CPC Class Codes: B01J 2219/00094 Jackets
• CPC Class Codes: B01J 2219/00135 Electric resistance heaters
• CPC Class Codes: B01J 2219/00155 using insulating materials or refractories
• CPC Class Codes: B01J 2219/00177 controlling the pH
• CPC Class Codes: B01J 2219/0018 controlling the conductivity
• CPC Class Codes: B01J 2219/0894 Processes carried out in the presence of a plasma
• CPC Class Codes: B22F 1/054 Nanosized particles
• CPC Class Codes: B22F 1/12 Metallic powder containing non-metallic particles containing lubricating or binding agents or organic material B22F1/10
• CPC Class Codes: B22F 2202/13 Use of plasma
• CPC Class Codes: B22F 2999/00 Aspects linked to processes or compositions used in powder metallurgy
• CPC Class Codes: B22F 9/12 starting from gaseous material
• CPC Class Codes: B29C 70/58 comprising fillers only , e.g. particles, powder, beads, flakes, spheres B29C70/025 takes precedence, agglomerating hollow spheres to produce synthetic foam B29C70/66; compounding ingredients per se C08K
• CPC Class Codes: B82B 1/00 Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
• CPC Class Codes: B82Y 25/00 Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: B82Y 5/00 Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
• CPC Class Codes: C01B 13/145 After-treatment of oxides or hydroxides, e.g. pulverising, drying, decreasing the acidity
• CPC Class Codes: C01B 19/007 : Tellurides or selenides of metals C01B19/002 takes precedence
• CPC Class Codes: C01B 21/062 : with chromium, molybdenum or tungsten
• CPC Class Codes: C01B 32/956 : Silicon carbide
• CPC Class Codes: C01B 35/04 : Metal borides
• CPC Class Codes: C01F 11/06 : of carbonates
• CPC Class Codes: C01F 5/06 : by thermal decomposition of magnesium compounds calcining magnesite or dolomite C04B2/10
• CPC Class Codes: C01G 23/006 : Alkaline earth titanates
• CPC Class Codes: C01G 41/02 : Oxides; Hydroxides
• CPC Class Codes: C01P 2002/01 : depicted by a TEM-image
• CPC Class Codes: C01P 2002/02 : Amorphous compounds
• CPC Class Codes: C01P 2002/34 : perovskite-type (ABO3)
• CPC Class Codes: C01P 2002/54 : one element only
• CPC Class Codes: C01P 2002/60 : Compounds characterised by their crystallite size
• CPC Class Codes: C01P 2002/72 : by d-values or two theta-values, e.g. as X-ray diagram
• CPC Class Codes: C01P 2004/03 : obtained by SEM
• CPC Class Codes: C01P 2004/04 : obtained by TEM, STEM, STM or AFM
• CPC Class Codes: C01P 2004/38 : cube-like
• CPC Class Codes: C01P 2004/51 : Particles with a specific particle size distribution
• CPC Class Codes: C01P 2004/54 : Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
• CPC Class Codes: C01P 2004/61 : Micrometer sized, i.e. from 1-100 micrometer
• CPC Class Codes: C01P 2004/62 : Submicrometer sized, i.e. from 0.1-1 micrometer
• CPC Class Codes: C01P 2004/64 : Nanometer sized, i.e. from 1-100 nanometer
• CPC Class Codes: C01P 2004/82 : two phases having the same anion, e.g. both oxidic phases
• CPC Class Codes: C01P 2006/10 : Solid density
• CPC Class Codes: C01P 2006/12 : Surface area
• CPC Class Codes: C01P 2006/40 : Electric properties
• CPC Class Codes: C01P 2006/60 : Optical properties, e.g. expressed in CIELAB-values
• CPC Class Codes: C01P 2006/80 : Compositional purity
• CPC Class Codes: C04B 2/10 : Preheating, burning calcining or cooling decarbonation during burning of cement raw materials C04B7/43; obtaining CaO or MgO otherwise than by thermal decomposition of the corresponding carbonates C01F11/02, C01F5/02
• CPC Class Codes: C04B 35/62222 : obtaining ceramic coatings coating of mortars, concrete, artificial or natural stone or ceramics C04B41/45; laminated ceramic products B32B18/00; coating metallic materials C23; coating of glass C03C17/00, applying ceramic coatings on silicon for semi-conductor purposes H01L
• CPC Class Codes: C04B 41/52 : Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
• CPC Class Codes: C04B 41/89 : for obtaining at least two superposed coatings having different compositions
• CPC Class Codes: C08J 5/005 : Reinforced macromolecular compounds with nanosized materials, e.g. nanoparticles, nanofibres, nanotubes, nanowires, nanorods or nanolayered materials
• CPC Class Codes: C08K 2201/011 : Nanostructured additives
• CPC Class Codes: C08K 3/01 : characterized by their specific function
• CPC Class Codes: C08K 3/08 : Metals
• CPC Class Codes: H01C 7/112 : ZnO type
• CPC Class Codes: H01F 1/0063 : in a non-magnetic matrix, e.g. granular solids granular films H01F10/007
• CPC Class Codes: H01G 4/12 : Ceramic dielectrics H01G4/085 takes precedence
• CPC Class Codes: H01G 4/33 : Thin- or thick-film capacitors thin- or thick-film circuits H01L27/00; capacitors without a potential-jump or surface barrier specially adapted for integrated circuits, details thereof, multistep manufacturing processes therefor H01L28/40
• CPC Class Codes: H01M 4/9066 : of metal-ceramic composites or mixtures, e.g. cermets
• CPC Class Codes: H01M 8/1213 : characterised by the electrode/electrolyte combination or the supporting material
• CPC Class Codes: H01M 8/1246 : the electrolyte consisting of oxides
• CPC Class Codes: H01M 8/1253 : the electrolyte containing zirconium oxide
• CPC Class Codes: Y02E 60/50 : Fuel cells
• CPC Class Codes: Y02P 40/40 : Production or processing of lime, e.g. limestone regeneration of lime in pulp and sugar mills
• CPC Class Codes: Y02P 70/50 : Manufacturing or production processes characterised by the final manufactured product
• CPC Class Codes: Y10S 977/89 : Deposition of materials, e.g. coating, cvd, or ald
• CPC Class Codes: Y10T 29/49002 : Electrical device making
• CPC Class Codes: Y10T 29/49082 : Resistor making
• CPC Class Codes: Y10T 428/26 : Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension

Abstract

Methods to manufacture nanoscale particles comprising metals, alloys, intermetallics, ceramics are disclosed. The thermal energy is provided by plasma, internal energy, heat of reaction, microwave, electromagnetic, direct electric arc, pulsed electric arc and/or nuclear. The process is operated at some stage above 3000K and at high velocities. The invention can be utilized to prepare nanopowders for nanostructured products and devices such as ion conducting solid electrolytes for a wide range of applications, including sensors, oxygen pumps, fuel cells, batteries, electrosynthesis reactors and catalytic membranes.

Claims

1. A process for manufacturing nanoscale powders comprising:

providing a feed comprising solid powders;

providing thermal energy to the feed to produce a vapor from the feed;

nucleating nanoscale powders from the vapor;

thermally quenching said nucleated nanoscale powders;

collecting the thermally quenched nanoscale powders, wherein the step of providing thermal energy raises a peak processing temperature to at least 3000 K; and

wherein the process operates at a peak processing velocity greater than 46 feet per second.

2. The process of claim 1 wherein the thermal energy is provided in the form of plasma.

3. The process of claim 1 wherein the thermal energy is provided in the form of internal energy.

4. The process of claim 1 wherein the thermal energy is provided in the form of pulsed electric arc.

5. The process of claim 1 wherein the thermal energy is provided in the form of a combination of two or more of methods selected from the group consisting of internal energy, heat of reaction, inductive, microwave, electromagnetic, direct electric arc, pulsed electric arc and nuclear.

6. The process of claim 1 wherein the nanoscale powders comprise an oxygen containing compound.

7. The process of claim 1 wherein the nanoscale powders comprise a metal containing compound.

8. The process of claim 1 wherein the nanoscale powers comprise a metal.

9. The process of claim 1 wherein the nanoscale powers comprise an alloy.

10. The process of claim 1 wherein the peak processing velocity is greater than 1 Mach.

21. The process of claim 1 wherein the nanoscale powders comprise a ceramic.

23. The process of claim 1 wherein the nanoscale powders comprise an intermetallic.

11. A process for manufacturing nanoscale powders comprising:

providing a feed comprising fluid;

providing thermal energy to the feed to produce a vapor from the feed;

nucleating nanoscale powders from the vapor;

thermally quenching said nucleated nanoscale powders;

collecting the thermally quenched nanoscale powders, wherein the step of providing thermal energy raises a peak processing temperature to at least 3000 K; and

wherein the process operates at a peak processing velocity greater than 46 feet per second.

12. The process of claim 11 wherein the thermal energy is provided in the form of plasma.

13. The process of claim 11 wherein the thermal energy is provided in the form of internal energy.

14. The process of claim 11 wherein the thermal energy is provided in the form of pulsed electric arc.

15. The process of claim 11 wherein the thermal energy is provided in the form of a combination of two or more of methods selected from the group consisting of internal energy, heat of reaction, inductive, microwave, electromagnetic, direct electric arc, pulsed electric arc and nuclear.

16. The process of claim 11 wherein the nanoscale powders comprise an oxygen containing compound.

17. The process of claim 11 wherein the nanoscale powders comprise a metal containing compound.

18. The process of claim 11 wherein the nanoscale powers comprise a metal.

19. The process of claim 11 wherein the nanoscale powers comprise an alloy.

20. The process of claim 11 wherein the peak processing velocity is greater than 1 Mach.

22. The process of claim 11 wherein the nanoscale powders comprise a ceramic.

24. The process of claim 11 wherein the nanoscale powders comprise an intermetallic.

25. A process for manufacturing nanoscale powders comprising:

providing a feed comprising a precursor in powder form suspended in a gas;

providing thermal energy to the feed thereby converting the precursor in powder form into a stream comprising vapor;

providing an extended reaction zone downstream of the step of providing thermal energy wherein the stream comprising vapor is condensed to nucleate solid nanoscale powders by adjusting the thermokinetic state of the stream comprising vapor;

providing a thermal quench of the solid nanoscale powders;

collecting the thermally quenched solid nanoscale powders;

wherein the step of providing thermal energy raises the peak processing temperature to at least 3000 K; and

wherein the process operates at a peak processing velocity greater than 46 feet per second.

26. The process of claim 25 wherein the thermal energy is provided in the form of plasma.

27. The process of claim 25 wherein the thermal energy is provided in the form of internal energy.

28. The process of claim 25 wherein the thermal energy is provided in the form of pulsed electric arc.

29. The process of claim 25 wherein the thermal energy is provided in the form of a combination of two or more of methods selected from the group consisting of internal energy, heat of reaction, inductive, microwave, electromagnetic, direct electric arc, pulsed electric arc and nuclear.

30. The process of claim 25 wherein the nanoscale powders comprise an oxygen containing compound.

31. The process of claim 25 wherein the

nanoscale powders comprise a metal containing compound.

32. The process of claim 25 wherein the nanoscale powders comprise a metal.

33. The process of claim 25 wherein the nanoscale powders comprise an alloy.

34. The process of claim 25 wherein the precursor in powder form suspended in a gas has a particle size greater than 1 micrometer.

35. The process of claim 25 wherein the gas comprises oxygen.

36. A process for manufacturing nanoscale powders comprising:

providing a feed comprising a precursor in powder form suspended in a gas;

providing thermal energy to the feed thereby converting the precursor in powder form into a stream comprising vapor;

providing an extended reaction zone downstream of the step of providing thermal energy thereby providing additional residence time to the stream comprising vapor;

providing an additional zone downstream of the extended reaction zone wherein the stream comprising vapor is condensed to nucleate solid nanoscale powders by adjusting the thermokinetic state of the stream comprising vapor;

providing a thermal quench of the solid nanoscale powders downstream of the additional zone;

collecting the thermally quenched solid nanoscale powders; and

wherein the gas is selected to provide an oxidizing or reducing atmosphere during the step wherein the precursor in powder form is converted into a stream comprising vapor.

37. The process of claim 36 wherein the peak processing velocity is greater than 1 Mach.

38. The process of claim 36 wherein the nanoscale powders comprise an intermetallic.

39. The process of claim 36 wherein the nanoscale powders comprise a ceramic.

40. The process of claim 36 wherein the nanoscale powders comprise a composite.

41. The process of claim 36 wherein the thermokinetic state of the stream comprising vapor is adjusted by addition of an oxidizing, reducing or inert kinetic gas in the additional zone.

42. The process of claim 36 wherein the thermokinetic state of the stream comprising vapor is adjusted by reducing the temperature of the stream to achieve supersaturation, wherein the supersaturation causes condensation of solid nanoscale powders in the additional zone.

43. The process of claim 42 wherein the condensed solid nanoscale powders have an average grain size less than 100 nm.

44. The process of claim 42 wherein the condensed solid nanoscale powders have an average grain size less than 50 nm.

45. The process of claim 42 wherein the condensed solid nanoscale powders have an average grain size less than 30 nm.

46. The process of claim 42 wherein the condensed solid nanoscale powders have an average grain size less than 20 nm.

47. The process of claim 36 wherein the thermokinetic state of the stream comprising vapor is adjusted to achieve control of one or more of desired characteristics of nanoscale powders and wherein the desired characteristics is selected from the group:

mean size of nanoscale powders, size distribution of nanoscale powders, phase of nanoscale powders, composition of nanoscale powders and interface of nanoscale powders.

48. The process of claim 36 wherein the gas used to suspend the precursor is selected to achieve control of one or more of desired characteristics of nanoscale powders and wherein the desired characteristics is selected from the group:

mean size of nanoscale powders, size distribution of nanoscale powders, phase of nanoscale powders, composition of nanoscale powders and interface of nanoscale powders.